水和土壤中磺胺和激素类药物的同时分析方法

Method for Simultaneous Determination of Sulfonamides and Hormone-Type Drugs in Water and Soil

建立了一种水和土壤中磺胺嘧啶、磺胺甲嘧啶、磺胺噻唑、磺胺二甲嘧啶、磺胺二甲氧嘧啶、磺胺甲唑6种磺胺类药物和17α-雌二醇、17β-雌二醇、雌酮、雌三醇、炔雌醇、乙烷雌酚6种激素类药物同时分析的方法。具体步骤:水样过滤后使用Oasis HLB固相萃取小柱进行净化富集;土壤样品经加速溶剂提取(ASE)之后过OasisHLB小柱净化富集;采用超高效液相色谱-串联质谱(UPLC-MS/MS)进行检测,分别以乙腈和1 mL.L-1甲酸溶液、乙腈和1 mL.L-1氨水溶液作为流动相。磺胺在水和土壤中的回收率分别为87.4%～103.6%和58.2%～80.0%,激素在水和土壤中的回收率分别为84.8%～101.8%和62.8%～79.3%,相对标准偏差均小于10.3%。水和土壤中磺胺的检测限分别为0.11～0.24 ng.L-1和0.01～0.02 ng.g-1,激素的检测限分别为0.31～2.14 ng.L-1和0.03～0.21 ng.g-1。用上述方法检测宿迁某典型养殖场周边的地表水和土壤,结果表明采用该方法检测环境样品中的磺胺和激素类药物是可行的。

A new method has been established for simultaneous determination of 6 sulfonamides, i.e. sulfadiazine, sulfa- merazine, sulfathiazole, sulfamethazine, sulfadimethazine, sulfamethoxazole, and 6 hormone-type drugs, i.e. 17α-estra-diol, 17β-estradiol, estrone, estriol, 17α-ethinyl-estradiol and hexestrol. Specific steps of the method are as following： After being filtered, water samples get purified and concentrated through Oasis HLB solid-phase extraction （SPE） cartrid- ges. After accelerated solvent extraction （ ASE）, soil samples get purified and concentrated through Oasis HLB cartridges. Then the water and soil samples are analyzed by UPLC-MS/MS, which uses solvent of acetonitrile-and-methanoic acid （ 1 mL·L- 1 ） and acetonitrile-and-ammonia （ 1mL ·L^-1） as mobile phase respectively. The mean recovery rate of sulfona- mides in water and soil samples varied in the range of 87.4% - 103.6% and 58.2% - 80. 0% , respectively, and that of the hormones in the range of 84. 8% - 101.8% and 62. 8% -79. 3%, respectively, with relative standard deviation all below 10. 3%. Detection limit of the method （MDL） for sulfonamides in water and soil ranged from 0. 11 to 0. 24 ng·L^-1 and from 0. 01 to 0. 02 ng·g^-1, respectively, and for the hormones did from 0. 31 to2. 14ng·L^-1 and from 0. 03 to 0. 21 ng·L^-1, respectively. This method was applied for determination of sulfonamides and hormones in the soil and sur-face water around a swine farm typical in Suqian area, with results demonstrating that this method is applicable to the determination of sulfonamides and hormone-type drugs in the environment.